© ISO 2017 Fertilizers and soil conditioners — Solid urea aldehyde slow release fertilizer — General requirements Engrais et amendements — Engrais urée aldéhyde solide à libération lente — Exigences g[.]
Trang 1Fertilizers and soil c onditioners —
Solid ur ea aldehyde slow release
En rais et amendement — En rais urée aldé yde solide à libération
lente — Exigence s g n rales
Fir t edition
2 17-0
Refer ence n mb r
Trang 2COPYRIGHT PROTECTED DOCUMENT
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written permis ion Permis ion c n be req esed from either ISO at the ad r es below or ISO’s member bod y in the c u try of
the r eq eser
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CH-1 14 Vernier, Geneva, Switzerlan
Tel + 12 7 9 011
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Trang 3F reword i v
Introduction v
1 Sc ope 1
2 Nor mati ve r eferenc es 1
3 Terms an definitions 1
4 Req irements 2
4.1 Visual inspe tion 2
4.2 Req ir ement of sold ur ea aldehyde slow r elease fe tilz r 2
5 A nal ytical metho s .3
5.1 Dete mination of the a pearanc 3
5.2 Dete mination of the mas fraction of total nitr og en 3
5.3 Dete mination of the mas fraction of ur eic nitrog en 3
5.4 Dete mination of the mas fraction of CWIN 3
5.4.1 Principle 3
5.4.2 Reag ents 3
5.4.3 A ppar atus 3
5.4.4 Pr oc d re 4
5.4.5 Ex pr es ion of results 4
5.5 Dete mination of the mas fraction of HWIN an A I 4
5.5.1 Principle 4
5.5.2 Reag ents 4
5.5.3 A ppar atus 5
5.5.4 Pr oc d re 5
5.5.5 Ex pr es ion of results 5
5.6 Dete mination of the mas fraction of nitr og en fr om IBDU an CDU 6
6 S mpl n and preparatio of test sample 6
6.1 Sampl ng method 6
6.1.1 Pr od cts in b g s 6
6.1.2 Pr od cts in bulk
6 6.2 Red ction of samples 6
6.3 Tes sample pr ep ration 6
7 Mar king and label ing 7
8 Packag ing, transport and storag e 7
Biblog raphy 8
Trang 4ISO (he Int ernational Org nization for Stan ardization) is a worldwidefede ation of national s an ards
b dies (ISO membe b dies) The work of pr p ring Int ernational Stan ards is normaly car ied out
through ISO t ech ical committ ees Each membe b dy int er st ed in a subje t for w hich a t ech ical
committ ee has be n es a lshed has the right t o be r pr sent ed on that committ ee Int ernational
org nizations, g ove nmental an non-g ove nmental, in laison with ISO, also take part in the work
ISO cola orat es closely with the Int ernational Ele trot ech ical C mmis ion (IEC) on al matt ers of
ele trot ech ical s an ardization
The proc d r s used t o develo this document an those int en ed for it furthe maint enanc ar
desc ibed in the ISO/IEC Dir ctives, Part 1 In p rticular the dife ent a pro al c it eria ne ded for the
dife ent ty es of ISO document should be not ed This document was draft ed in ac ordanc with the
edit orial rules of the ISO/IEC Dir ctives, Part 2 ( e www iso org dir ctives)
A tt ention is drawn t o the p s ibi ity that some of the element of this document ma be the subje t of
p t ent right ISO shal not be held r sponsible for identifying any or al such p t ent right Detais of
any p t ent right identified d ring the develo ment of the document wi be in the Introd ction an / r
on the ISO ls of p t ent de larations r c ived ( e www iso org p t ent )
Any trade name used in this document is information given for the convenienc of use s an does not
cons itut e an en orsement
F or an ex lanation on the v lu tary natur of s an ards, the meaning of ISO spe if ic t erms an
ex r s ions r lat ed t o conformity as es ment, as wel as information a out ISO’ s adhe enc t o the
World Trade Org nization (WTO) principles in the Te hnical Bar ie s t o Trade (TBT) se the folowing
URL: www iso org iso / for word html
This document was pr p r d b Te h ical Committ ee ISO/TC 1 4, Fertii ze s a d soi c onditio e s
Trang 5Sold ur a aldehyde slow r lease fe ti iz r is a non-co t ed an chemicaly synthesiz d nitrog en
fe ti z r with slow r lease efe t In 1 24, the f irs slow r lease fe ti z r p t ent in the world was
is ued t o ur a formaldehyde (UF) an in 1 5 , UF was put int o comme cial prod ction as the oldes
slow r lease fe ti z r Sold ur a aldehyde slow r lease fe ti iz r has the long es hist ory of r sear h,
use an prod ction among the slow r lease fe ti z rs used in practic A t the same time, it is the mos
widely used of al slow r lease fe ti iz rs
F or faci tating int ernational fe ti z r trade, it is ne es ary t o ha e an int ernational an g ene al
s an ard for sold ur a aldehyde slow r lease fe ti iz rs
Trang 7Fertilizers and soil c onditioners — Solid urea aldehyde
This document spe ifies g ene al r q ir ment , analytical methods, sampl ng an pr paration of t es
sample, marking an la el ng, packa ing, transport an st orag e for sold ur a aldehyde slow r lease
fe ti z r
This document a ples t o pur sold ur a aldehyde slow r lease fe ti iz r, i.e ur a formaldehyde (UF),
methy lene ur a (MU), c ot ony lidene diur a (CDU), iso uty lidene diur a (IBDU) This document does
not a ply t o mixtur s of nitrog enous fe ti z rs containing sold ur a aldehyde slow r lease fe ti z r
2 Normati ve r eferences
The folowing document ar r fe r d t o in the t ext in such a wa that some or al of their cont ent
cons itut es r q ir ment of this document F or dat ed r fe enc s, only the edition cit ed a ples F or
un at ed r fe enc s, the lat es edition of the r fe enc d document ( inclu ing any amen ment ) a ples
ISO 5 1 , Fertii ze s — Dete min tio o total nitro en c ontent — Titrimetric meth d ate di s ti atio
ISO 740 , Fertii ze s — Markin — Pres entatio a d declarations
ISO 741 , Fertii ze s a d s oi c onditio e s — Fin l s amples — Prac tic al ar a gement
ISO 7 42, S ld fertii ze s — R educ tio o s amples
ISO 8 5 , Fertii ze s a d soi c onditio e s — Voc ab lar y
ISO 86 3, S ld fertii ze s — Simple s ampln meth d fr s mal lots
ISO 1 746:2 1 , Dete min tio o ur a c ontent in ur a-b sed fertii ze s b hig pe frma ce lq id
chromato ra h (HPLC)
ISO 2 7 5:2 1 , Fertii ze s — Dete min tio o ur a c ondens ates us in hig -pe frma c e lq id
chromato ra h (HPLC) — Isob t yldenediur a a d c roto yldenediur a (meth d A ) a d meth len-ur a
olg me s (meth d B)
3 Terms and definitions
F or the purposes of this document, the t erms an def initions given in ISO 8 5 and the folowing a ply
ISO an IEC maintain t erminolo ical data ases for use in s an ardization at the folowing ad r s es:
— IECEle tro edia: a aia le at ht p:/ www ele tro edia org
— ISO Onlne brow sing plat orm:a ai a le at ht ps:/ www iso org o p/
3.1
ure aldehy e slow rele se fertiizer
prod ct of r action betwe n ur a an aldehyde()that prod c a slow r lease nitrog enous fe ti iz r
E AMP E Ure formaldehyde (UF), meth lene ure (MU), c oton lidene diure (CDU), iso utylidene
diure (IBDU)
Trang 8cold water insolu le nitrog en
CWIN
insoluble nitrog en fractions in ur a formaldehyde or methy lene ur a prod ct that ar insoluble in
phosphat e bufe solution (pH7,5) or dis i ed wat er at 2 °Cd ring a 1 min pe iod
3.3
cold water soluble nitrog en
CWSN
soluble nitrog en fractions in ur a formaldehyde or methy lene ur a prod ct that ar soluble in
phosphat e bufe solution (pH7,5) or dis i ed wat er at 2 °Cd ring a 1 min pe iod
Not e 1t o entry: CW SN= Total nitrog en – CWIN
3.4
hot water insolu le nitrog en
HWIN
insoluble nitrog en fractions in ur a formaldehyde or methy lene ur a prod ct that ar insoluble in
phosphat e bufe solution (pH7,5) at 1 0 °C d ring a 3 min pe iod
3.5
hot water soluble nitrog en
soluble nitrog en fractions in ur a formaldehyde or methy lene ur a prod ct that ar soluble in
phosphat e bufe solution (pH7,5) at 1 0 °C d ring a 3 min pe iod
Not e 1t o entry: HW SN = Total nitro en – HWIN
3.6
hot water soluble nitrog en o ly
HWSN o ly
soluble nitrog en fractions in ur a formaldehyde or methy lene ur a prod ct that ar soluble in
phosphat e bufe solution (pH 7,5) at 1 0 °C d ring a 3 min pe iod an insoluble in phosphat e bufe
solution (pH7,5) at 2 °C d ring a 1 min pe iod
Not e 1t o entry: HW SN only =HW SN – CW SN = CWIN – HWIN
3.7
activity index
AI
pe c ntag eof CWIN (3.2)that is solubi ised in hot wat er ( HWSN o ly) (3.6)
Not e 1t o entry: A I=
CWIN HW IN
CWIN
−
×1 0
Not e 2t o entry: CWIN an HWIN in Not e 1are e pres ed in the mas fraction (% )
Not e 3t o entry: A higher AI in icat es b t er slow rele se characteristic of ure formaldehyde fertilizer
4.1 Visual inspection
The prod ct shal be in p wde , gran les, pri s, pelet , p s i les, chips or othe sold forms V isualy
inspe t for the pr senc of contaminant an for ign matt er
4.2 Requirement of sol d ur ea aldehyde slow release fer ti izer
Sold ur a aldehyde slow r lease fe ti z r shal be t est ed t o demons rat e conformanc with al the
r q ir ment spe if ied in Ta les 1 an 2 r spe tively, an de lar d v lues on containe s
Trang 9Table 1 — Requirements of ure formaldehy e/methy lene ure ferti izer
3 5of the declared t otal
nitro en content
The req irement spe if ied b national/regional legislation shal be folowed when ure formaldehyde meth lene ure s
are c vered b legislation
Table 2— Requirements of IBDU and CDU
The req irement spe if ied b the national/regional legislation shal be folowed when IBD or CD are c vered b
legislation
5 A nal ytical methods
5.1 Determination of the appe ranc e
It shal be det ermined b visual method
5.2 Determination of the mas fraction of total nitrog en
It shal be det ermined in ac ordanc with ISO 5 1
5.3 Determination of the mas fraction of ureic nitr og en
It shal be det ermined in ac ordanc with ISO 1 746
5.4 Determination of the mas fraction of CWIN
5.4.1 Principle
Extraction of the t es p rtion in phosphat e bufe solution (pH 7,5) or dis i led wat er at 2 °C Fitration
of insoluble r sid e, washing an det ermination of nitrog en cont ent in insoluble r sid e
5.4.2 Re g ents
5.4.2.1 Phosphate bufe solutio (pH 7,5) Dis olve 14,3 g KH
2 PO
4
an 91,0 g K
2 HPO
4
in wate an
di ute to 1 l Diute 1 0ml of this solution to 1 l
5.4.2.2 A nhydr ous ethanol
5.4.2.3 Reag ent ls ed in ISO 5 1
5.4.3 A pparatus
Trang 105.4.3.2 Wate bath, ca a le of being maintained at (2 ± 2)°C.
5.4.3.3 Q uantitati ve fi ter paper (inte mediate spe d)
5.4.3.4 A pp ratus ls ed in ISO 5 1
5.4.4 Proc edure
Two analyses shal be pe formed simultaneously for the det ermination
Plac 1 g t o 1,4 g t es p rtion (ac urat e t o 0,0 0 1 g) in 5 ml beake wet with ethanol (5.4.2.2) A dd
2 ml phosphat e bufe solution (5.4.2.1) or dis i led wat er an let s an 1 min in the wat er b th
maintained at 2 °C ± 2 °C an s ir at 5 min int erv ls d ring s an ing Trans e the supe nat e t o a pie e
of filt er p pe (5.4.3.3) in a long -st em fu nel an wash the r sid e four or f ive times b de anting with
wat er of 2 °C ± 2 °C Finaly, trans e al the r sid e t o the f ilt er p pe an complet e washing u ti the
filtrat e measur s 2 0 ml Det ermine nitrog en cont ent in the filt er p pe and the r sid e in ac ordanc
with ISO 5 1
Car y out a blank t es at the same time as the det ermination, using the same proc d r , using the same
r ag ent , but omit ing the t es portion
5.4.5 Ex pres io of results
The CWIN cont ent, w
1 , ex r s ed as a mas fraction (% ), is given b F ormula (1):
w
m 1
1
140
10 0
1 0
=
×
×
(1)
w he e
V
1
is the v lume, in mi l itr s, of sodium hydro ide s an ard solution used for the blank t est ;
V
2
is the v lume, in mi l itr s, of sodium hydro ide s an ard solution used for the
det ermination;
c
1
is the conc ntration, in mol pe ltr , of sodium hydro ide s an ard solution used;
m
1
is the mas , in grams, of the t es portion
The calculation r sult ar ac urat e t o two digit aft er the de imal p int The det ermination r sult is
the arithmetic a e ag e of thed plcat e det ermination r sult
5.5 Deter mination of the mas fraction of HWIN and A I
5.5.1 Pr inciple
Extraction of the t es p rtion in phosphat e bufe solution (pH 7,5) at 1 0 °C Fi tration of insoluble
r sid e, washing an det ermination of nitrog en cont ent in insoluble r sid e
5.5.2 Re g ents
5.5.2.1 Reag ent ls ed in 5.4.2
5.5.2.2 Cel te
Trang 115.5.3 A pparatus
5.5.3.1 Usual labor ator y apparatus
5.5.3.2 Water bath, ca a leof being maintained at (1 0 ± 2) °C
5.5.3.3 A pp ratus ls ed in 5.4.3.3an 5.4.3.4
5.5.4 Pr oc edure
Two analy ses shal be pe formed simultaneously for the det ermination
Plac an ac urat ely weighed t es p rtion containing 0,1 g CWIN (ac urat e t o 0,0 0 1 g) in a 2 0 ml tal
-form beaker A dd 1 0ml 1 0 °C phosphat e bufe solution (5.4.2.1) from a grad at ed cy lin e t o the t es
p rtion, s ir, co e an imme se promptly in a b i ing wat er b th (5.5.3.2) so that lq id in the beaker
is below the wat er level in the wat er bath Maintain the wat er b th at 9 °C t o 1 0 °C, che k with a
the momet er an s ir at 1 min int erv ls Aft er ex ctly 3 min, r mo e the beake from the wat er b th
an f ilt er promptly through a pie e of filt er p pe (5.4.3.3) If f iltration takes mor than 4 min, discard
det ermination R epeat the det ermination, ad ing 1 g c l t e (5.5.2.2) as filt er-aid jus befor r mo ing
the beaker from the wat er bath, s ir an f ilt er
Wash the insoluble r sid e complet ely ont o the f ilt er p pe with b i ing wat er an contin e washing
unti the t otal v lume used is 1 0 ml C mplet e washing befor the f iltrat e be omes clou y or it
t empe atur dro s t o below 6 °C Det ermine t otal nitrog en in the wet f ilt er p pe an r sid e in
ac ordanc with ISO 5 1
Car y out a blan t es at the same time as the det ermination, using the same proc d r and r ag ent ,
but omit ing the t es protion
5.5.5 Ex pr es ion of r esults
5.5.5.1 HWIN c ontent of the sample
The HWIN cont ent, w
2 , ex r s ed as a mas fraction ( % ), is given b F ormula (2):
w
m 2
2
14 0
10 0
1 0
=
×
×
(2)
w he e
V
3
is thev lume, in mi l itr s, of sodium hydro ide s an ard solution used for the blank t est ;
V
4
is thev lume, in mi l itr s, of sodium hydro ide s an ard solution used for the
det ermination;
c
2
is theconc ntration, in mol pe ltr s, of sodium hydro ide s an ard solution used;
m
2
is themas , in grams, of the t es portion
The calculation r sult ar ac urat e t o two digit aft er the de imal p int The det ermination r sult is
the arithmetic a e ag e of the d plcat e det ermination r sult
Trang 125.5.5.2 Calculation of A I
AI, ex r s ed in %, is given b F ormula (3):
A I=
w
1
1 0
−
5.6 Deter mination of the mas fraction of nitr og en from IBDU and CDU
It shal be det ermined in ac ordanc with ISO 2 7 5:2 1 , method A or ISO 1 746
6 Sampl ng and pr eparation of test sample
6.1 S mpl ng method
6.1.1 Products in bag s
Car y out the samplng o e ation b folowing the proc d r desc ibed in ISO 8 3
6.1.2 Products in bulk
Car y out the samplng o e ation b folowing the proc d r desc ibed in ISO 8 3
6.2 Reduction of samples
Mix al the inc ement (cole t ed as in 6.1) u iformly an promptly t o form a single a gr g t e sample
using a devic or b han The a gr g t e sample is r d c d t o a out 1 kg ac ording t o the proc d r
in ISO 7 42 Next, divide int o two part for final la orat ory samples The two la orat ory samples ar
put int o two clean an dry glas or plas ic containe s or any othe ine t mat erial of adeq at e r sis anc
ca a le of maintaining the sample in it original con ition The containe s shal be fitt ed with airtight
closur s C r y out al the o e ations desc ibed a ove as ra idly as p s ible t o a oid los or g in of
mois ur Each containe shal be se ur d an sealed folowing the ins ruction given in ISO 741 Each
la orat ory sample shal be la eled folowing the ins ructions given in ISO 741 The la el shal, at
minimum, car y the folowing information:
a) thename of man factur r;
b) thename of prod ct ;
c) theman factur r’s r fe enc an b t ch n mbe or prod ction dat e ( if a ai a le);
d) thelot siz ;
e) thedat e of samplng;
f) theplac ofsampl ng;
g) thesignatur of the sample ;
h) the signatur an name of the pe son or his r pr sentative on whose pr mises the sample w as taken
One of thecontaine s is used for furthe q alty analy sis, w hie the othe is kept for ad itional analy sis
in 6 mos
6.3 Test sample preparation
S le t one of the la orat ory samples from the two containe s o tained in 6.2 Mix the cont ent of the
containe ac ording t o the proc d r in ISO 7 42 The t es sample used for det ermining the it ems